反应 #2391

反应方程式

4-tert-butyl-N-{6-[2-(5-methylsulfinylpyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide

→

4-tert-butyl-N-{6-[2-(5-mercaptopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide

收率 118.4%

溶剂

trifluoroacetic anhydride

methylene chloride

反应条件

后处理

1. 1
   其他the mixture is evaporated
2. 2
   其他to remove the solvent
3. 3
   workup.DISSOLUTIONThe residue is dissolved in methanol/triethylamine (1:1) (20 ml)
4. 4
   浓缩concentrated to dryness under reduced pressure
5. 5
   workup.DISSOLUTIONThe residue is dissolved in chloroform
6. 6
   洗涤washed with saturated aqueous ammonium chloride solution and brine
7. 7
   干燥dried over sodium sulfate
8. 8
   过滤filtered
9. 9
   浓缩The filtrate is concentrated under reduced pressure

实验过程

A solution of 4-tert-butyl-N-{6-[2-(5-methylsulfinylpyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide (471 mg) in trifluoroacetic anhydride (5 ml) and methylene chloride (5 ml) is refluxed for 30 minutes, and the mixture is evaporated to remove the solvent. The residue is dissolved in methanol/triethylamine (1:1) (20 ml), and concentrated to dryness under reduced pressure. The residue is dissolved in chloroform, washed with saturated aqueous ammonium chloride solution and brine, dried over sodium sulfate, and filtered. The filtrate is concentrated under reduced pressure to give 4-tert-butyl-N-{6-[2-(5-mercaptopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide as pale yellow foam (529 mg).

来源